Cyclical method of producing high-purity nitrogen and optionally a high-purity hydrocarbon from a feedstock containing nitrogen and a hydrocarbon

a technology of high-purity hydrocarbons and feedstocks, which is applied in the direction of separation processes, chemical/physical/physico-chemical processes, and dispersed particle separation, etc., can solve the problems of high cost of methods, low yield, and often inability to recycle nitrogen and hydrocarbons in the process

Active Publication Date: 2015-09-17
TOTAL RES & TECH FELUY +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

[0011]The process which is a subject matter of the invention makes it possible, starting from a simple and inexpensive installation, to separate a nitrogen / hydrocarbons mixture in order to recover either high-purity nitrogen or, simultaneously, high-purity nitrogen and high-purity hydrocarbons, this being achieved with excellent degrees of recovery.
[0050]a line which makes it possible to recycle said fraction of propylene and propane with a purity≧95 mol % in the polymerization reactor or else a distillation column in order to separate the propylene from the propane starting from said fraction.

Problems solved by technology

The mixture of nitrogen and hydrocarbons often cannot be recycled in the process.
However, the method is expensive and yields are generally low.
However, these processes require bulky installations with high operating expenses (OPEX) and capital expenses (CAPEX).
However, the adsorption capacity of these adsorbents is insufficient to compete with the industrial processes described above.

Method used

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  • Cyclical method of producing high-purity nitrogen and optionally a high-purity hydrocarbon from a feedstock containing nitrogen and a hydrocarbon
  • Cyclical method of producing high-purity nitrogen and optionally a high-purity hydrocarbon from a feedstock containing nitrogen and a hydrocarbon
  • Cyclical method of producing high-purity nitrogen and optionally a high-purity hydrocarbon from a feedstock containing nitrogen and a hydrocarbon

Examples

Experimental program
Comparison scheme
Effect test

example 1

1) Example 1

Measurements of Equilibrium and Simulation

[0066]FIG. 1 represents the adsorption isotherms for nitrogen on MIL-100(Fe) as characterized in Table 2 at different temperatures (50, 100 and 150° C.), up to 5 bar abs., measured in a Rubotherm magnetic suspension balance.

[0067]FIG. 2 represents the comparison between the adsorption isotherms for nitrogen and propylene at 50° C. on MIL-100(Fe) as characterized in Table 2.

[0068]It emerges from these isotherms that the propylene / nitrogen selectivity at 1 bar abs. and 50° C. is approximately 40.

[0069]Two cyclical PSA processes were simulated:[0070]A) process for production of high-purity nitrogen from a nitrogen / propylene mixture,[0071]B) process for production of high-purity nitrogen, on the one hand, and of high-purity propylene, on the other hand, from a nitrogen / propylene mixture.

[0072]The nitrogen / propylene mixture comprises 70 mol % of nitrogen and 30 mol % of propylene. It is introduced into the adsorbent bed under the foll...

example 2

2) Example 2

Experiment at the Pilot Scale

[0090]The dynamic adsorption capacity (dynamic capacity) of the MIL-100(Fe) with respect to propylene was determined at 50° C. and 70° C.

[0091]Furthermore, adsorption / desorption cycles in VPSA (Vacuum Pressure Swing Adsorption) mode were carried out in order to experimentally confirm the simulation results described above.

2.1. Description of the Pilot Plant

[0092]The pilot plant is composed of nitrogen and liquid propylene storage tanks, of a regulator which makes it possible to regulate the nitrogen flow rate, of a positive displacement pump intended for the liquid propylene and of an evaporator located over the mixture, upstream of the adsorption column. The adsorbent (MIL-100(Fe) as described below) bed is placed in the adsorption column with an internal diameter of 1″ and with a height of 2 m. This column is equipped with an external jacket in which a temperature-regulated heat-exchange fluid capable of operating between 20 and 200° C. cir...

example 3

3) Example 3

Measurements of Equilibrium on MIL-125(Ti)_NH2 or UiO-66(Zr)

[0135]FIG. 8 represents the comparison between the adsorption isotherm for nitrogen and the adsorption isotherm (black points) and desorption isotherm (white points) for propylene at 70° C. over MIL-125(Ti)_NH2, the characteristics of which are shown in the following table 10.

[0136]FIG. 9 represents the comparison between the adsorption isotherm for nitrogen and the adsorption isotherm (black points) and desorption isotherm (white points) for propylene at 70° C. over UiO-66(Zr).

TABLE 10MIL-125 (Ti)_NH2UiO-66(Zr)Form of the adsorbentPowderPowderPorosity0.59cc / g0.8cc / gBET specific surface1450m2 / g1350m2 / g

[0137]The sorption isotherms were measured using a device of IGA (Intelligent Gravimetric Analyzer, Hiden Analytical Ltd.) type with control of the pressure of the gas (0-5 bar) at 70° C. Before carrying out the adsorption measurements, the samples of adsorbent (30 mg) were dehydrated at 200° C. for 12 hours under ...

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Abstract

The invention relates to a cyclical method for producing a nitrogen fraction, the purity of which is greater than or equal to 95 mol %, and a hydrocarbon-enriched fraction from a filler containing nitrogen and a hydrocarbon, said method using a specific class of porous hybrid solids as an adsorbent in a pressure-swing adsorption (PSA) process. The invention also relates to equipment for implementing said method.

Description

RELATED APPLICATIONS[0001]The present application is a National Phase entry of PCT Application No. PCT / EP2012 / 075676, filed Dec. 14, 2012, which claims priority from U.S. Patent Application No. 61 / 710,333, filed Oct. 5, 2012, said applications being hereby incorporated by reference herein in their entirety.FIELD OF THE INVENTION[0002]The present invention relates to a cyclical process for the production of a nitrogen fraction with a purity of greater than or equal to 95 mol % (2), on the one hand, and of a fraction enriched in hydrocarbon (3), on the other hand, from a feedstock (1) comprising nitrogen and a hydrocarbon, and also to an installation for the implementation of this process.BACKGROUND OF THE INVENTION[0003]There exist many processes in the energy industry, the refining industry or the petrochemical industry during which a mixture of nitrogen and hydrocarbon(s) is formed. For example, during the production of polypropylene from propylene, nitrogen is used to purify the p...

Claims

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Application Information

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Patent Type & Authority Applications(United States)
IPC IPC(8): B01D53/047C08F110/06
CPCB01D53/0476C08F110/06B01D2253/204B01D2257/702B01D2256/24B01D2259/4003B01D2256/10B01D2257/102C08F6/005B01D2257/7022B01D2259/40001B01D2259/40022B01D2259/40066B01D2259/403B01D2259/404B01J2219/00006C01B21/0455C10G25/003C10G25/12C10G50/00C10G57/02C10G2300/202B01J20/226B01J20/28066B01J20/3491B01J20/3425B01J20/28073C08L23/10
Inventor LUCK, FRANCISLEROI, CATHERINEFERNANDEZ, ALVAROPEIXOTO RIBEIRO, ANA MAFALDA ALMEIDAGODINHO DE FARIA DOS SANTOS, JOAO CARLOSRODRIGUES, ALIRIO EGIDIOCHANG, JONG-SANLEE, U-HWANGHWANG, YOUNG KYUBONNE, JEAN-PATRICK
Owner TOTAL RES & TECH FELUY
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